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At least 307 records · Page 17
All sourcesNASA NTRSDOE OSTI
DOE OSTI2016

Cold Sintering Process of Composites: Bridging the Processing Temperature Gap of Ceramic and Polymer Materials

Co-sintering ceramic and thermoplastic polymer composites in a single step with very high volume fractions of ceramics seems unlikely, given the vast differences in the typical sintering temperatures of ceramics versus polymers. These processing limitations are overcome with the introduction of a new sintering approach, namely “cold sintering process” (CSP). CSP utilizes a transient low temperature solvent, such as water or water with dissolved solutes in stoichiometric ratios consistent with the ceramic composition, to control the dissolution and precipitation of ceramics and effect densification between room temperature and ≈200 °C. Under these conditions, thermoplastic polymers and ceramic materials can be jointly formed into dense composites. Three diphasic composite examples are demonstrated to show the overall diversity of composite material design between organic and inorganic oxides, including the microwave dielectric Li 2 MoO 4 –(-C 2 F 4 -) n , electrolyte Li 1.5 Al 0.5 Ge 1.5 (PO 4 ) 3 –(-CH 2 CF 2 -) x [-CF2CF(CF3)-] y, and semiconductor V 2 O 5 –poly(3,4-ethylenedioxythiophene) polystyrene sulfonate composites. Cold sintering is more general and shall have a major impact on the processing of composite materials for many different applications, mechanical, thermal, and electronic, to mention a few possibilities. CSP concepts open up new composite material design and device integration schemes, impacting a wide variety of applications.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Investigation of Thermal Conductivities and Expansion Coefficients of (Yb{sub 1 − x}La{sub x}){sub 2}AlTaO{sub 7} Ceramics

The (Yb{sub 1 − x}La{sub x}){sub 2}AlTaO{sub 7} (x = 0, 0.1, 0.3, 0.5) ceramics were prepared by solid-state reaction method. The phase composition, microstructure, thermophysical properties of (Yb{sub 1 − x}La{sub x}){sub 2}AlTaO{sub 7} ceramics were investigated. Results reveal that (Yb{sub 1 − x}La{sub x}){sub 2}AlTaO{sub 7} (x = 0, 0.1, 0.3) ceramics exhibit a single pyrochlore-type structure, and the (Yb{sub 0.5}La{sub 0.5}){sub 2}AlTaO{sub 7} has an orthorhombic weberite structure. The thermal conductivities of (Yb{sub 1 − x}La{sub x}){sub 2}AlTaO{sub 7} (x = 0, 0.1, 0.3) ceramics decrease with increasing Yb{sub 2}O{sub 3} contents. (Yb{sub 0.5}La{sub 0.5}){sub 2}AlTaO{sub 7} has the highest thermal conductivity among all the ceramics studied, within the range of 1.48-1.75 W/m K (20-1200 °C). The thermal expansion coefficients of (Yb{sub 1 − x}La{sub x}){sub 2}AlTaO{sub 7} ceramics decrease gradually with increasing La{sub 2}O{sub 3} fractions, and the thermal expansion coefficients are close to those of YSZ.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Effect of Sintering Atmosphere on the Synthesis Process, Electrical and Mechanical Properties of NiFe{sub 2}O{sub 4}/Nano-TiN Ceramics

NiFe{sub 2}O{sub 4}/nano-TiN ceramics were fabricated by a two-step cold-pressing sintering process. Effect of sintering atmosphere (air, nitrogen, argon) on the synthesis process of NiFe{sub 2}O{sub 4}/nano-TiN ceramics was investigated. The DSC-TG and XRD analysis results indicated that besides principal phases of NiO and NiFe{sub 2}O{sub 4}, new-phase Ni{sub 3}TiO{sub 5} formed in the sintered ceramics under the three sintering atmospheres, and metallic phase including iron and nickel appeared in the sintered samples with inert gas (nitrogen, argon) sintering condition. Microstructure analysis results showed that considerable quantity of micropores appeared in the ceramic samples sintered under inert gases (argon, nitrogen), but lower porosity (3.0, 3.6%) and higher densities (4.78 g/cm{sup 3}, 4.51 g/cm{sup 3}) can be obtained, comparing to the both values (14.4%, 4.17 g/cm{sup 3}) for the ceramic samples sintered under air atmosphere. Besides, the average bending strength and elastic modulus of the samples sintered under argon is 113.75 MPa and 7.13GPa, which is higher than that of 75.12 MPa, 5.42GPa and 91.96 MPa, 6.26GPa for the samples synthesized under air and nitrogen, separately. When changing sintering atmosphere from air to inert gases (argon, nitrogen), the fracture model of the 4 wt.%nano-TiN/NiFe{sub 2}O{sub 4} ceramics synthesized at 1400 °C for 4 h transformed from intergranular fracture to intergranular-transgranular fracture.

36 MATERIALS SCIENCE↗
DOE OSTI2020

A review of composite polymer-ceramic electrolytes for lithium batteries

All solid-state lithium batteries are garnering attention in both academia and industry. Lithium-ion conductive polymers and lithium-ion conductive ceramics are the two major classes of solid electrolytes that have prevalently been pursued for many years. However, each of them has its own advantages and disadvantages. One approach to overcome the disadvantages and get the best out of each of those materials is a solid composite electrolyte that combines the advantages of inorganic ceramic electrolytes and solid polymer electrolytes. Such composite electrolytes can offer acceptable ionic conductivity, high mechanical strength, and favorable interfacial contact with electrodes, which can greatly improve the electrochemical performance of all-solid-state batteries compared to cells based on a polymer electrolyte alone or a ceramic electrolyte alone. We present in this review the state-of-the-art composite polymer-ceramic electrolytes in view of their electrochemical and physical properties for the applications in lithium batteries. The review mainly encompasses the polymer matrices, various ceramic filler materials, and the polymer/ceramics composite systems. Specifically, the structures, ionic conductivities, electrochemical/chemical stabilities, and fabrications of solid composite electrolytes are discussed in-depth. On the basis of previous work, a perspective on future research directions is highlighted for developing high-performance composite polymer-ceramic electrolytes.

25 ENERGY STORAGE↗
DOE OSTI2014

Electrical properties of (1−x)(Bi{sub 0.5}Na{sub 0.5})TiO{sub 3}–xKNbO{sub 3} lead-free ceramics

In this investigation, a simple compound (1−x)(Bi{sub 0.5}Na{sub 0.5})TiO{sub 3}–xKNbO{sub 3} (BNT–xKN, x=0–0.08) lead-free ceramics were synthesized successfully by conventional solid state reaction method. The piezoelectric, dielectric and ferroelectric characteristics of the ceramics were investigated and discussed. The results shows that moderate KN addition can enhance the piezoelectric response without an obvious decline of ferroelectric properties. The largest piezoelectric response is obtained in BNT–0.05KN, whereas largest electric-field-induced strain is obtained in BNT–0.06KN. An effective d{sub 33}{sup eff} of ∼400 pC/N calculated from electric-field-induced strain is obtained in BNT–0.06KN. The present investigation demonstrates that addition KN effectively reduces the depolarization temperature of the BNT–xKN ceramics. The electrical properties of the ceramics are tightly related to their depolarization temperature. - Graphical abstract: Unipolar electric-field-induced strain for the BNT–xKN ceramics. A maximum strain of 0.28% is achieved with a low field in BNT–0.06KN. - Highlights: • Moderate KNbO{sub 3} addition enhances the piezoelectric properties of the ceramics. • A maximum strain of 0.28% is achieved with a low field. • A large piezoelectric response is achieved in 0.95(Bi{sub 0.5}Na{sub 0.5})TiO{sub 3}–0.05KNbO{sub 3}. • The electrical properties are tightly related to the depolarization temperature T{sub d}.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Formation mechanism and characteristics of lanthanum-doped BaTiO{sub 3} powders and ceramics prepared by the sol–gel process

Pure and lanthanum-doped barium titanate nanopowders described by two different formulae, as Ba{sub 1−x}La{sub x}TiO{sub 3}, for lower La concentrations (0 ≤ x ≤ 0.005) and Ba{sub 1−x}La{sub x}Ti{sub 1−x/4}O{sub 3} for higher La concentration (x = 0.025) were prepared by an alkoxide sol–gel method. Single phase compositions were obtained after annealing at 900 °C for 2 h, in air. The increase of the lanthanum content causes structural and morphological changes in the oxide powders, including the evolution of the unit cell from tetragonal toward a cubic symmetry, the particle size decrease and a higher aggregation tendency. SEM investigations of the ceramics sintered at 1300 °C for 4 h indicate significant changes of the microstructural features (strong decrease of the average grain size and increase of the intergranular porosity) with the raise of La amount. Lanthanum addition to barium titanate prepared by sol–gel induces a more significant shift of the Curie temperature toward lower values, than that one reported in literature for ceramics of similar compositions, but processed by the conventional solid state method. The compositions with smaller La amount (x ≤ 0.005) show semiconducting properties at room temperature and high relative dielectric permittivity values, while the undoped ceramics and those doped with higher La content (x = 0.025) are good dielectrics. The ceramic with x = 0.025 exhibits acceptable low losses, a very diffuse ferroelectric–paraelectric transition and Curie temperature closed to the room temperature, being thus susceptible for high tunability applications. - Highlights: • Ba{sub 1−x}La{sub x}TiO{sub 3} (x ≤ 0.005) and Ba{sub 1−x}La{sub x}Ti{sub 1−x/4}O{sub 3} (x = 0.025) were prepared by sol–gel. • Ceramics with x < 0.5 exhibit semiconductor and high dielectric properties. • Ceramic with x = 0.025 exhibits acceptable low losses and diffuse phase transition.

36 MATERIALS SCIENCE↗
DOE OSTI2013

High Schottky barrier at grain boundaries observed in Na{sub 1/2}Sm{sub 1/2}Cu{sub 3}Ti{sub 4}O{sub 12} ceramics

Graphical abstract: - Highlights: • NSCTO exhibits a high ε′ of 7.0–8.4 × 10{sup 3} and low tan δ of 0.030–0.041. • NSCTO exhibits a high E{sub b} of ∼2208 V cm{sup −1} and large α of 15.6. • Giant ε′ response is attributed to the electrically heterogeneous microstructure. • High Φ{sub b} values at grain boundaries are found to be 0.925–0.964 eV. • Formation of a potential barrier at grain boundaries is caused by Schottky effect. - Abstract: The dielectric properties and nonlinear current–voltage characteristics of Na{sub 1/2}Sm{sub 1/2}Cu{sub 3}Ti{sub 4}O{sub 12} ceramics prepared by a conventional solid state reaction method were investigated. Na{sub 1/2}Sm{sub 1/2}Cu{sub 3}Ti{sub 4}O{sub 12} ceramics exhibited a high dielectric permittivity of 7.0–8.4 × 10{sup 3} and low loss tangent (tan δ∼0.030–0.041). Non-Ohmic properties with a high breakdown voltage of ∼2208 V cm{sup −1} and large nonlinear coefficient of 15.6 were observed in Na{sub 1/2}Sm{sub 1/2}Cu{sub 3}Ti{sub 4}O{sub 12} ceramics. Using complex impedance analysis, Na{sub 1/2}Sm{sub 1/2}Cu{sub 3}Ti{sub 4}O{sub 12} ceramics were shown to be electrically heterogeneous consisting of semiconducting grains and insulating grain boundaries. Giant dielectric properties were described based on the electrically heterogeneous microstructure. X-ray photoelectron spectroscopy analysis suggested that the semiconductive nature of grains may be related to the presence of Cu{sup +} and Ti{sup 3+}. The formation of an electrostatic potential barrier at the grain boundaries of Na{sub 1/2}Sm{sub 1/2}Cu{sub 3}Ti{sub 4}O{sub 12} ceramics was suggested to be caused by the Schottky effect. Interestingly, high electrostatic potential barriers at grain boundaries in Na{sub 1/2}Sm{sub 1/2}Cu{sub 3}Ti{sub 4}O{sub 12} ceramics were calculated and found to be 0.925–0.964 eV.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Origin of giant dielectric constant and conductivity behavior in Zn{sub 1−x}Mg{sub x}O (0 ≤ x ≤ 0.1) ceramics

Highlights: • Mg doped zinc oxide ceramics were fabricated by co-precipitation/solid state reaction. • MZO ceramics shown a Debye type and colossal dielectric response. • Physical absorption of atmospheric water vapor contributes these high permittivity. • The fabricated ceramic shows Maxwell–Wagner type of relaxation. - Abstract: Zn{sub 1−x}Mg{sub x}O ( ≤ x ≤ 0.1) ceramics were fabricated by conventional solid-state reaction of co-precipitated zinc oxide and magnesium hydroxide nanoparticles. Structural and morphological properties of the fabricated ceramics were studied using X-ray diffraction and scanning electron microscopic analysis. The dielectric measurements of the ceramics were carried out as a function of frequency and temperature respectively. Interestingly, Mg doped ZnO (MZO) samples exhibited colossal dielectric response (∼1 × 10{sup 4} at 1 kHz) with Debye like relaxation. The detailed dielectric studies and thermal analyses showed that the unusual dielectric response of the samples were originated from the defected grain and grain boundary (GB) conductivity relaxations due to the absorbed atmospheric water vapor (moisture). Impedance spectroscopy was employed to determine the defected grain and GB resistances, capacitances and which supported Maxwell–Wagner type relaxation phenomena.

36 MATERIALS SCIENCE↗
DOE OSTI2016

The enhancing performance of (Ba{sub 0.85}Ca{sub 0.15}Ti{sub 0.90}Zr{sub 0.10})O{sub 3} ceramics by tuning anatase–rutile phase structure

Graphical abstract: Titanium dioxide (TiO{sub 2}) with different phase structure had interesting influence on the crystal structure, microstructure, the sintering temperature and electrical properties. - Highlights: • BCZT ceramics were prepared using either anatase or rutile structures as Ti source. • Orthorhombic and tetragonal mixture structure was exhibited by adjusting Ti source. • The optimal properties were observed in BCZT ceramics with rutile titanium dioxide. - Abstract: To research effect of raw materials TiO{sub 2} with the phase structures on the crystal structure, microstructure and electrical properties of lead-free (Ba{sub 0.85}Ca{sub 0.15})(Ti{sub 0.90}Zr{sub 0.10})O{sub 3} (BCZT) ceramics, BCZT ceramics using either anatase or rutile as Ti source were synthesized by solid-state reaction. Titanium dioxide (TiO{sub 2}) with anatase/rutile phase structures had interesting influence on the crystal structure, microstructure and the sintering temperature by the X-ray diffraction and SEM, which also played an important role in improved electrical properties. The BCZT ceramics with rutile titanium dioxide demonstrated optimal piezoelectric and dielectric properties: d{sub 33} = 590 pC/N, k{sub p} = 0.46, ε{sub r} = 2810, tanδ = 0.014 and T{sub c} = 91 °C, which was obviously superior to BCZT ceramics with anatase titanium dioxide.

36 MATERIALS SCIENCE↗
DOE OSTI2018

High thermal stability and excellent dielectric properties of a novel X8R-type CdCu3Ti4O12 ceramics through a sol-gel technique

Highlights: • CdCu{sub 3}Ti{sub 4}O{sub 12} (CdCTO) ceramics were successfully synthesized via the sol-gel method, and the optimized processing parameters were obtained. • The outstanding dielectric properties: ε{sub r} ≈ 1.63 × 10{sup 4} and tan δ = 0.035 (at 10 kHz) could be obtained in CdCTO ceramics sintered at 1000 °C. • The CdCTO-SG ceramics obtained an excellent thermal stability. - Abstract: CdCu{sub 3}Ti{sub 4}O{sub 12} (CdCTO) ceramics were systematically synthesized via the sol-gel technique. The optimal CH{sub 3}COOH and Ti(OC{sub 4}H{sub 9}){sub 4} concentrations in the synthesis solution and processing temperature were found to be 5.0 vol%, 0.50 mol/L and 60 °C, respectively. These materials exhibited high densities and fine-grained microstructures along with outstanding dielectric properties, including an ε{sub r} of approximately 1.63 × 10{sup 4} and a tan δ of 0.035 at 10 kHz. Over the temperature range from −55 to 150 °C, the temperature coefficients of the dielectric constant at 1 and 10 kHz were −13.9% to 1.20% and −9.10% to 3.92%, respectively, indicating that these ceramics possess excellent thermal stability. These properties also meet the requirements for X8R applications. Data acquired from complex impedance spectroscopy and electrical modulus assessments demonstrates that the superior dielectric properties of these CdCTO ceramics can be attributed to the internal barrier layer capacitor theory (IBLC).

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Synthesis and microwave dielectric characteristics of high-Q Li2MgxTiO3+x ceramics system

Highlights: • A laminated sintering technique was adopted to prevent lithium volatilization. • The sintering behavior and microwave dielectric properties of Li{sub 2}Mg{sub x}TiO{sub 3+x} (2.2 ≤ x ≤ 4) ceramics were investigated. • The Li{sub 2}Mg{sub 3.6}TiO{sub 6.6} ceramics had excellent microwave dielectric properties of ε{sub r} ∼ 12.7, Q × f ∼ 169,000 GHz, τ{sub f} ∼ −32.8 ppm/°C. - Abstract: High-Q Li{sub 2}Mg{sub x}TiO{sub 3+x} (2.2 ≤ x ≤ 4) microwave dielectric ceramics were fabricated by using a conventional solid-state reaction method followed by laminated sintering technique. All samples showed clear and smooth grains through this sintering method. The XRD patterns indicated that Li{sub 2}Mg{sub x}TiO{sub 3+x} (2.2 ≤ x ≤ 4) ceramics displayed MgO-like cubic phase with ordered rock salt structure. The dielectric constant decreased monotonically because the molar volume expanded and molecular polarizability decreased when x values increased. The Q × f values of Li{sub 2}Mg{sub x}TiO{sub 3+x} (2.2 ≤ x ≤ 4) ceramics were dependent significantly on both average grain sizes and packing fraction. The Li{sub 2}Mg{sub 3.6}TiO{sub 6.6} ceramics sintered at 1375 °C had excellent microwave dielectric properties of ε{sub r} ∼ 12.7, Q × f ∼ 169,000 GHz, τ{sub f} ∼ −32.8 ppm/°C.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

SrV2O6: An ultralow-firing microwave dielectric ceramic for LTCC applications

Highlights: • α-SrV{sub 2}O{sub 6} and β-SrV2O{sub 6} phase were coexisted below 500 °C, and stable α-SrV{sub 2}O{sub 6} phase at 630 °C. • Optimum microwave dielectric properties: ε{sub r} ∼9.66, Q × f ∼23,200 GHz, and τ{sub f} ∼ −205 ppm/°C were obtained. • CaTiO{sub 3} successfully adjusted τ{sub f} value toward to near-zero with −2.7 ppm/°C. • Their chemical compatibility with the aluminum electrodes were evaluated. - Abstract: A novel ultralow-firing microwave dielectric ceramic SrV{sub 2}O{sub 6} was prepared at 630 °C through the solid-state method. Phase evolution and crystal structure were analyzed by XRD and Raman spectroscopy. Results show that α-SrV{sub 2}O{sub 6} and β-SrV{sub 2}O{sub 6} phase coexisted when fired at lower temperatures (α-SrV{sub 2}O{sub 6} phase was obtained at 550 °C and remained stable up to 660 °C. Optimum microwave dielectric properties with a quality factor ∼23,200 GHz, a low dielectric constant ∼9.66, and a temperature coefficient of resonant frequency ∼−205 ppm/°C was obtained. SrV{sub 2}O{sub 6} ceramic possessed chemical compatibility with aluminum electrodes when cofired at 630 °C. The temperature stability of SrV{sub 2}O{sub 6} was adjusted by forming composite ceramics with CaTiO{sub 3} and a near-zero τ{sub f} ∼−2.7 ppm/°C was achieved in the 0.75SrV{sub 2}O{sub 6}-0.25CaTiO{sub 3} ceramic. All the results show that the SrV{sub 2}O{sub 6} ceramic might be a promising candidate as substrates in ultra-low temperature cofired (ULTCC) ceramics.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Enhanced piezoelectric properties in (Ba1-xCax)(Ti0.90Sn0.10)O3-0.08Dy2O3 lead-free ceramics

Highlights: • MPB exists in the BCTSD ceramics with x = 0.06–0.10. • BCTSD ceramics exhibit typical diffuse phase transition behavior, which is not sensitive to the amount of Ca{sup 2+} ions. • Remarkable improvement on piezoelectric properties (d{sub 33} = 675 pC/N, k{sub p} = 55%) were achieved at x = 0.06. - Abstract: (Ba{sub 1-x}Ca{sub x})(Ti{sub 0.90}Sn{sub 0.10})O{sub 3}-0.08Dy{sub 2}O{sub 3} ceramics (BCTSD-x, x = 0.02–0.10) were fabricated by conventional solid state sintering method. The effect of Ca{sup 2+} ions addition on the phase structure, microstructure, and electric properties of ceramics were studied. X-ray diffraction analysis reveals the replacement of Ba{sup 2+} ions in the perovskite structure by Ca{sup 2+} ions. Rhombohedral phase and tetragonal phase coexist in the composition with x = 0.06–0.10. Both d{sub 33} and K{sub p} of the ceramics increase with increasing Ca concentration, and attain maximum values of 675 pC/N and 55.0%, respectively, for x = 0.06. All the ceramics present typical diffuse phase transition behavior, and the feature is not sensitive to the amount of Ca{sup 2+} ions.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Critical role of polymer-ceramic ion exchange for high conductivity composite electrolytes

Polymer-ceramic composites offer a path to enhance the transport and mechanical properties of solid electrolytes. However, an in-depth understanding of the extent and role of ion transport along and across polymer-ceramic interfaces in these systems is lacking. We have recently shown that Li-conducting Li 0.11 Na 0.24 K 0.02 La 0.43 TiO 2.82 (LMTO) nanorods can be prepared by a molten flux method, and the addition of 30–50 weight (wt.)% LMTO to a bis[(trifluoromethyl)sulfonyl]imide-vinyl ethylene carbonate-based single-ion conducting (SIC) polymer electrolyte leads to a two-fold enhancement in Li-ion conductivity, from 1.4 to 3.0 × 10 −5 S/cm at 30 °C. In the present study, we use NMR methods to identify the Li-ion transport pathways and determine the timescale of chemical exchange between the SIC polymer and LMTO ceramic components. Tracer exchange NMR indicates preferential transport through the polymer or polymer-interfacial regions, and exchange spectroscopy (EXSY) and a new isotope exchange method reveal negligible Li exchange between the SIC polymer and LMTO ceramic up to several days. Here, LMTO nanorods act as a passive filler. Our results further highlight that significant (e.g., 10- or 100-fold) conductivity enhancements in composite electrolytes can only be achieved 1) with ionically-conductive fillers, and 2) when both the ceramic and polymer components actively participate in long-range transport. For this, fast interfacial ion exchange is needed. In conclusion, this leads us to introduce a critical interfacial ion exchange time to evaluate whether a filler actively contributes to conduction in a composite electrolyte, and screen for promising polymer-ceramic pairings to accelerate the development of high conductivity solid electrolytes.

Battery, Solid electrolyte↗
DOE OSTI2015

Development of a sintering process for recycling oil shale fly ash and municipal solid waste incineration bottom ash into glass ceramic composite

Highlights: • Glass ceramic composite is prepared from oil shale fly ash and MSWI bottom ash. • A novel method for the production of glass ceramic composite is presented. • It provides simple route and lower energy consumption in terms of recycling waste. • The vitrified slag can promote the sintering densification process of glass ceramic. • The performances of products decrease with the increase of oil shale fly ash content. - Abstract: Oil shale fly ash and municipal solid waste incineration bottom ash are industrial and municipal by-products that require further treatment before disposal to avoid polluting the environment. In the study, they were mixed and vitrified into the slag by the melt-quench process. The obtained vitrified slag was then mixed with various percentages of oil shale fly ash and converted into glass ceramic composites by the subsequent sintering process. Differential thermal analysis was used to study the thermal characteristics and determine the sintering temperatures. X-ray diffraction analysis was used to analyze the crystalline phase compositions. Sintering shrinkage, weight loss on ignition, density and compressive strength were tested to determine the optimum preparation condition and study the co-sintering mechanism of vitrified amorphous slag and oil shale fly ash. The results showed the product performances increased with the increase of sintering temperatures and the proportion of vitrified slag to oil shale fly ash. Glass ceramic composite (vitrified slag content of 80%, oil shale fly ash content of 20%, sintering temperature of 1000 °C and sintering time of 2 h) showed the properties of density of 1.92 ± 0.05 g/cm{sup 3}, weight loss on ignition of 6.14 ± 0.18%, sintering shrinkage of 22.06 ± 0.6% and compressive strength of 67 ± 14 MPa. The results indicated that it was a comparable waste-based material compared to previous researches. In particular, the energy consumption in the production process was reduced compared to conventional vitrification and sintering method. Chemical resistance and heavy metals leaching results of glass ceramic composites further confirmed the possibility of its engineering applications.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2013

Ferroelectric, piezoelectric, and dielectric properties of BiScO{sub 3}-PbTiO{sub 3}-Pb(Cd{sub 1/3}Nb{sub 2/3})O{sub 3} ternary high temperature piezoelectric ceramics

(0.95-x)BiScO{sub 3}-xPbTiO{sub 3}-0.05Pb(Cd{sub 1/3}Nb{sub 2/3})O{sub 3} (BS-xPT-PCN) high temperature piezoelectric ceramics near the morphotropic phase boundary (MPB) have been synthesized by traditional solid-state reaction methods. The microstructural morphology, phase structure, and electrical properties of BS-xPT-PCN ceramics were investigated in detail. X-ray diffraction analysis indicated BS-xPT-PCN ceramics have a pure perovskite structure. The coexistence of rhombohedral and tetragonal phases at MPB composition enhanced the polarizability by the coupling between two dynamically equivalent energy states, resulting in the improved piezoelectric and ferroelectric properties at MPB vicinity. The BS-xPT-PCN (x = 0.60) ceramics possess the optimal piezoelectric and ferroelectric properties with d{sub 33} = 505pC/N, k{sub p} = 55.9%, k{sub t} = 36.5%, strain = 0.23% (under the electric field 37.5 kV/cm), and P{sub r} = 39.7 {mu}C/cm{sup 2}. High temperature dielectric behaviors showed diffuse phase transition in BS-xPT-PCN ceramics. The Curie temperature T{sub c} was found to increase from 371 Degree-Sign C to 414 Degree-Sign C with x increasing from 0.58 to 0.62. All these results together with the good thermal stabilities make the BS-xPT-PCN ceramics promising candidates for high temperature piezoelectric applications.

36 MATERIALS SCIENCE↗
DOE OSTI2013

The Cr-substitution concentration dependence of the structural, electric and magnetic behaviors for Aurivillius Bi{sub 5}Ti{sub 3}FeO{sub 15} multiferroic ceramics

Aurivillius Bi{sub 5}Ti{sub 3}FeO{sub 15} (BTFO) multiferroic ceramics with different Cr-doped concentrations have been synthesized by the conventional solid state reaction method. The influences of Cr-doping concentrations on the structural, magnetic, dielectric, and ferroelectric properties of BTFO ceramics are investigated in detail. All these sintered Cr-substituted BTFO ceramics are determined to be layered perovskite Aurivillius structure by X-ray diffraction, as well as the lattice parameters a, b, and c are in good accordance with Vegard's law along with the Cr-doping concentration. The lattice distortion a/b for Aurivillius family decreases with increasing Cr-doping concentration. Moreover, Cr-doping can promote greatly the grain growth of BTFO samples confirmed from field emission scanning electron microscopy characterization. However, no obvious signs of the improvement in ferroelectric properties are found in Cr-doped BTFO ceramics, and abnormal ferroelectric polarization versus electric field (P-E) loops are observed as Cr-doping content is beyond 0.1. Similar ε (tanδ) versus frequency plots to those of the BTFO sample are exhibited when Cr-doping concentration is less than 0.1. Nevertheless, obvious dielectric dispersion phenomena are shown as the Cr-doping concentration is beyond 0.1, and this dispersion behavior becomes strong with further increasing Cr-doping concentration, which are clearly indicated by the appearance of dielectric loss relaxation peaks in the measurement frequency from 10{sup 2} Hz to 10{sup 6} Hz. In addition, the corresponding frequency to relaxation peak shifts towards high frequencies with the Cr-doping concentration. Finally, the same magnetic orderings for all these Cr-doped BTFO ceramics as those of the BTFO one, i.e., superparamagnetic state dominated with antiferromagnetic interaction, are unambiguously found, signifying that the predicted Fe{sup 3+}-O-Cr{sup 3+} 180° ferromagnetic superexchange interaction based on the Goodenough-Kanamori (G-K) rule might not be achieved in BTFO ceramics through Cr substitution by the conventional solid state reaction.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Investigations of Ba{sub x}Sr{sub 1−x}TiO{sub 3} ceramics and powders prepared by direct current arc discharge technique

Ba{sub x}Sr{sub 1−x}TiO{sub 3} ceramics with x ranging from 0 to 1 were prepared by direct current arc discharge technique and studied by means of x-ray diffraction (XRD) and Raman spectroscopy. The cubic-tetragonal ferroelectric phase transition in Ba{sub x}Sr{sub 1−x}TiO{sub 3} ceramics was found to occur at x ≈ 0.75. XRD investigation of as-grown BaTiO{sub 3} ceramics revealed co-existence of tetragonal and hexagonal modifications with a small amount of impurity phase BaTi{sub 4}O{sub 9}. No evidences of hexagonal phase were observed in Raman spectra of as-grown BaTiO{sub 3} ceramics, while Raman peaks related to hexagonal phase were clearly observed in the spectrum of fine-grain powders prepared from the same ceramics. A core-shell model for BaTiO{sub 3} ceramics prepared by direct current arc discharge technique is proposed. Absence of the hexagonal phase in any Ba{sub x}Sr{sub 1−x}TiO{sub 3} solid solution with x < 1 is discussed in the frame of specific atomic arrangement.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗